CN109799299A - A kind of quick environmental protection tests method of free fatty acid methyl esters and ethyl ester in olive oil - Google Patents
A kind of quick environmental protection tests method of free fatty acid methyl esters and ethyl ester in olive oil Download PDFInfo
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Abstract
The present invention provides a kind of quick environmental protection tests method of free fatty acid methyl esters and ethyl ester in olive oil, belongs to field of food detection.The quick environmental protection tests method includes the following steps: (1) using silicagel column SupelcleanTMLC-Si SPE carries out pre-treatment to olive oil sample；(2) olive oil sample after pre-treatment is analyzed using gas-chromatography；(3) content of free fatty acid methyl esters and ethyl ester in olive oil is calculated according to working curve.Detection method, pretreatment process is easy, quick, the use for the organic solvent being largely harmful to the human body can be saved, it can be achieved that low cost and environmental protection purpose, in addition analysis time is short, accurately and reliably, high sensitivity.
Description
Technical field
The present invention relates to the quick environmental protection tests methods of free fatty acid methyl esters in a kind of olive oil and ethyl ester, belong to food
Detection field, especially food adulteration detection field.
Background technique
Olive oil (OliveOil) is using the fruit of olive tree as the grease of waste.It is different according to processing technology,
Virgin oil and Marc oil can be divided into, virgin oil can be divided into different brackets again, wherein seeking with Extra Virgin
Support value highest.China is edible oil big country, and with economic development, China is continuously increased the demand of olive oil, only 2017
Year aggregate consumption is about 600,000 tons, wherein 80% relies on import.
However, China consumer is limited to olive oil eries product understanding, and Extra Virgin yield is few, price
It is high.Dealer in order to promote the sale of products and reap staggering profits, to olive oil be exaggerated publicity or with bad the phenomenon that substituting the bad for the good it is commonplace.
Especially almost nominal " Extra Virgin ", total amount are total considerably beyond global Extra Virgin without exception for the olive oil of import
Yield.This shoddy olive oil not only serious infringement equity of consumer, it is also possible to which the body for influencing consumer is strong
Health.
Therefore, olive oil level identification is established, the method for especially Extra Virgin level identification consumes guarantee
Person's equity and strike malfeasance have great importance.
The methanol and ethyl alcohol generated in the fermentation process of olive can react with fatty acid, generate free fatty acid
The content of methyl esters and ethyl ester, higher grade olive oil free fatty acid methyl esters and ethyl ester can be lower and with free fatty acid methyl
Based on ester type compound.So the fatty-acid ethyl ester content≤35mg/kg that dissociates in Extra Virgin is required in international standard,
And the requirement to the not no index of other grade olive oil.
Therefore, it is easy, quick, environmentally friendly to establish pretreatment process, high-throughput, highly sensitive and high accuracy detection side
Method, so as to realize the level identification of Extra Virgin, provided effectively for the strike adulterated doping behavior of olive oil industry
The demand of foundation is extremely urgent.
Summary of the invention
The object of the present invention is to provide the quick environmental protection tests method of free fatty acid methyl esters in a kind of olive oil and ethyl ester,
Pretreatment process is easy, quick, can save the use for the organic solvent being largely harmful to the human body, it can be achieved that low cost and environmental protection
Purpose, in addition analysis time is short, accurately and reliably, high sensitivity.
The purpose of the present invention adopts the following technical scheme that realization.
The quick environmental protection tests method of free fatty acid methyl esters and ethyl ester, includes the following steps: in a kind of olive oil
(1) silicagel column Supelclean is usedTMLC-Si SPE carries out pre-treatment to olive oil sample；
(2) olive oil sample after pre-treatment is analyzed using gas-chromatography；
(3) content of free fatty acid methyl esters and ethyl ester in olive oil is calculated according to working curve.
In the present invention, the free fatty acid methyl esters include methyl hexadecanoate, methyl stearate, methyl oleate, sub- oil
Sour methyl esters, the free-fat acetoacetic ester include ethyl palmitate, ethyl stearte, ethyl oleate, ethyl linoleate.
In the present invention, olive oil sample is transferred to the silicagel column activated in advance with 6mL n-hexane with 1-3mL n-hexane
In, chromatography eluant is carried out with the mixed liquor of 25-30mL n-hexane and ether, collects eluent, solvent is removed, then uses 1-3mL
N-hexane dissolution.
In the present invention, gas chromatography analysis method is as follows: after analyzing pre-treatment using DB-5HT gas chromatography
Olive oil sample；Capillary column temperature program: initial temperature be 80 DEG C, rise to 140 DEG C with 40 DEG C/min heating rate, then with
5 DEG C/min heating rate rises to 335 DEG C, and in 335 DEG C of holding 20min；Injector temperature: 250 DEG C；Detector temperature: 350
℃；Carrier gas: helium；Flow rate of carrier gas: 1.0mL/min；Sample volume: 1.0 μ L；Input mode: Splitless injecting samples.
In the present invention, the working curve obtains with the following method: n-hexane being used to contain palm for solvent preparation
Sour methyl esters, methyl stearate, methyl oleate, methyl linoleate, ethyl palmitate, ethyl stearte, ethyl oleate and linoleic acid
The mixed mark standard working solution I of ethyl ester；The mixed mark standard working solution I is diluted to the mixed mark of several various concentrations using n-hexane
Standard working solution；Each mixed mark standard working solution is analyzed using gas-chromatography, using each aliphatic ester content as abscissa, with
The gas-chromatography peak area of each aliphatic ester is ordinate mapping, draws working curve.
Gas chromatography analysis method is as follows during obtaining working curve: using the mixed mark of DB-5HT gas chromatography analysis
Standard working solution；Capillary column temperature program: initial temperature be 80 DEG C, rise to 140 DEG C with 40 DEG C/min heating rate, then with
5 DEG C/min heating rate rises to 335 DEG C, and in 335 DEG C of holding 20min；Injector temperature: 250 DEG C；Detector temperature: 350
℃；Carrier gas: helium；Flow rate of carrier gas: 1.0mL/min；Sample volume: 1.0 μ L；Input mode: Splitless injecting samples.
In the present invention, olive oil sample is added to before preceding processing and takes myristic acid methyl esters and methyl margarate.
The present invention also provides above-mentioned detection methods in olive oil answering in free fatty acid methyl esters and ethyl ester qualitative detection
With.
Method provided by the invention, pretreatment process is easy, quick, can save the organic solvent being largely harmful to the human body
Use, it can be achieved that low cost and environmental protection purpose, in addition analysis time is short, accurately and reliably, high sensitivity.It is provided by the invention
The detection of method free fatty acid methyl esters and ethyl ester suitable for olive oil, for grade, the strike for identifying Extra Virgin
The adulterated doping behavior of olive oil industry provides effective foundation.
Detailed description of the invention
Fig. 1 is the gas chromatogram of mixed mark standard working solution I.
Fig. 2 is the gas chromatogram of free fatty acid methyl esters in Extra Virgin (FAME) and ethyl ester (FAEE).
Fig. 3 is the gas chromatogram of free fatty acid methyl esters in virgin oil (FAME) and ethyl ester (FAEE).
Fig. 4 is the gas chromatogram of free fatty acid methyl esters in mixed olive oil (FAME) and ethyl ester (FAEE).
Fig. 5 is gas chromatogram of the olea europaea fruit residual oil middle reaches from fatty acid methyl ester (FAME) and ethyl ester (FAEE).
Specific embodiment
Embodiment 1 establishes the detection method of free fatty acid methyl esters and ethyl ester in olive oil
1. the preparation of standard reserving solution
It accurately weighs respectively myristic acid methyl esters (Methyl myristate, No. CAS: 124-10-7 is denoted as C14:0M), palm fibre
Palmitic acid acid methyl esters (Methyl palmitate, No. CAS: 112-39-0 is denoted as C16:0M), ethyl palmitate (Ethyl
Palmitate, No. CAS: 628-97-7 is denoted as C16:0E), methyl margarate (Methyl heptadecanoate, CAS
Number: 1731-92-6 is denoted as C17:0M), methyl linoleate (Methyl linoleate, No. CAS: 112-63-0 is denoted as C18:
2M), methyl oleate (Methyl oleate, No. CAS: 112-62-9 is denoted as C18:1M), methyl stearate
(Methylstearate, No. CAS: 112-61-8 is denoted as C18:0M), ethyl linoleate (Ethyl linoleate, No. CAS:
544-35-4 is denoted as C18:2E), ethyl oleate (Ethyl oleate, No. CAS: 111-62-6 is denoted as C18:1E) and stearic acid
Ethyl ester (Ethylstearate, No. CAS: 111-61-5 is denoted as C18:0E) each 1mg of standard items (being accurate to 0.01mg), is placed in
In 10mL volumetric flask, with n-hexane dissolution and it is settled to graduation mark, being configured to the reference substance list mark stock solution of 1mg/mL, (4 DEG C cold
Hiding saves, and validity period is 1 year).
1mL C16:0M, C16:0E, C18:2M, C18:1M, C18:0M, C18:2E, C18:1E and C18:0E are drawn respectively
Single mark stock solution is settled to graduation mark with n-hexane, being made into each material concentration is 100 μ g/ into the same 10mL volumetric flask
The mixed mark standard solution I of mL.The mono- mark stock solution of C14:0M and C17:0M of 1mL is drawn into the same 10mL volumetric flask, with just
Hexane is settled to graduation mark, and being made into two kinds of material concentrations is the mixed mark standard solution II of 100 μ g/mL, to judge detection method
Stability and reliability (4 DEG C stored refrigerated, and validity period is 6 months).
2. the preparation of standard working solution
The mixed mark standard solution I of 100 μ g/mL of 1mL is drawn, until it is settled to graduation mark with n-hexane in 10mL volumetric flask,
It is made into the mixed mark standard working solution I that each material concentration is 10 μ g/mL.C14 containing 10 μ g/mL is prepared using same method:
The mixed mark standard working solution II of the C17:0M of 0M and 10 μ g/mL.Mixed mark standard working solution I and mixed mark standard working solution II are cold at 4 DEG C
Hiding saves, and validity period is 6 months.
3. the pre-treatment of sample
Olive oil sample 0.05g (being accurate to 0.0001g) is accurately weighed in 10mL teat glass, 50 each substances of μ L are added
Concentration is the mixed mark standard working solution II of 10 μ g/mL (for assisting to judge the stability and reliability of detection method).With just
Olive oil sample is transferred to the commercialization silicagel column (U.S. activated in advance with 6mL n-hexane by hexane (point 2 total 2mL)
Supelco company, SupelcleanTMLC-Si SPE, amount of silica gel 500mg) in, with the mixing of 25mL n-hexane and ether
Liquid (volume ratio of n-hexane and ether is 99: 1) carries out chromatography eluant, and flow velocity is about to drip for every 10 seconds 15, collects eluent.
Above-mentioned isolated eluent is concentrated with 45 DEG C of water-baths of rotary evaporator, until solvent almost removes, add 2mL just oneself
Alkane, concussion dissolution take redissolution object to cross the organic phase filter membrane that aperture is 0.45 μm, the olive oil sample after obtaining pre-treatment.
4. gas chromatographic analysis
Olive after pre-treatment is analyzed using DB-5HT gas chromatography (30m × 0.25mm × 0.25 μm, Agilent)
Oil samples.Wherein, capillary column temperature program: initial temperature is 80 DEG C, rises to 140 DEG C with 40 DEG C/min heating rate, then
335 DEG C are risen to 5 DEG C/min heating rate, and in 335 DEG C of holding 20min；Injector temperature: 250 DEG C；Detector temperature: 350
℃；Carrier gas: helium (purity >=99.999%)；Flow rate of carrier gas: 1.0mL/min；Sample volume: 1.0 μ L；Input mode: it does not shunt
Sample introduction.
5. chromatographic peak is identified
Peak each in sample is identified using external standard method qualitative method, i.e., by the guarantor at peak each in olive oil sample
It stays the time to be compared with mark standard working solution I is mixed under same analysis condition, each fatty acid methyl ester and ethyl ester is identified, if
Retention time is consistent, then is substance of the same race.
If existing and C14:0M and C17:0M retention time in mixed mark standard working solution II on the chromatogram of olive oil sample
Consistent substance, it was demonstrated that detection method stability is good, high reliablity.
6. the detection method range of linearity, detection limit and quantitative limit measurement
A certain amount of mixed mark standard working solution I (each material concentration is 10 μ g/mL) is drawn, is diluted to n-hexane and is
Mixed mark standard working solution (concentration is respectively 0.1 μ g/mL, 0.2 μ g/mL, 0.5 μ g/mL, 1 μ g/mL and 2 μ g/mL) of column, in this reality
It applies in a title 4 and is analyzed under GC conditions.Using each aliphatic ester content as abscissa (X), the gas phase color of each aliphatic ester
Spectral peak area is ordinate (Y) mapping, draws working curve, obtains regression equation.Each rouge is calculated according to S/N=3 and S/N=10
The detection limit (LOD) and quantitative limit (LOQ), standard substance gas chromatogram of fat acid esters are detailed in Fig. 1, and as a result see Table 1 for details.
Linear equation, related coefficient, detection limit and the quantitative limit of 1 free fatty acid methyl esters of table and ethyl ester
The above results show: the working curve linear relationship of each aliphatic ester is good, and detection limit and quantitative limit are below
4.0mg/kg is able to satisfy free fatty acid methyl esters and the requirement of ethyl ester limit detection in olive oil.
7. detecting the specific method of olive oil sample
Pre-treatment is carried out to olive oil sample using method in the present embodiment title 3, using method in the present embodiment title 4
It is detected.
Peak each in sample is identified using external standard method qualitative method, i.e., by the guarantor at peak each in olive oil sample
The time is stayed to be compared with mark standard working solution I is mixed under same analysis condition, if retention time is consistent, for substance of the same race.
The calculating of fatty acid methyl ester or ethyl ester concentration is as follows in sample: by integrator, measure corresponding fatty acid methyl ester and
The peak area of ethyl ester calculates the content (μ g/mL) of each fatty acid methyl ester or ethyl ester in measurement liquid according to working curve；Then it presses
Column formula calculates each fatty acid methyl ester and ethyl ester content in olive oil sample:
K=(X × V)/m
In formula:
The content of aliphatic ester in K-olive oil sample, unit are milligrams per kilogram (mg/kg)；
Aliphatic ester content in X-measurement liquid, unit are every milliliter of milligram (μ g/mL)；
The last constant volume of V-test sample, unit are milliliter (mL)；
M-olive oil sample quality, unit are gram (g).
According to international standard, free fatty acid methyl esters and ethyl ester are in olive oil with methyl hexadecanoate (C16:0M), palmitinic acid
Ethyl ester (C16:0E), methyl linoleate (C18:2M), methyl oleate (C18:1M), methyl stearate (C18:0M), linoleic acid second
Ester (C18:2E), ethyl oleate (C18:1E) and ethyl stearte (C18:0E) totally eight kinds of aliphatic ester summation meters.
Embodiment 2 detects the rate of recovery and essence of fatty acid methyl ester and ethyl ester content in olive oil sample using the method for the present invention
Density
24 parts of samples are taken from same Extra Virgin sample, every part of 0.05g is equally divided into 4 groups, every group of 6 parts of samples
Product.1st group carries out pre-treatment by 1 title 3 of embodiment, is then detected by the method for 1 title 4 of embodiment；2-4 group is used for
Mixed mark standard working solution I (1 title 2 of embodiment, the concentration 10 of 25 μ L is added in mark-on reclaims test in the 2nd group of every part of sample
μ g/mL), the mixed mark standard working solution I of 50 μ L is added in the 3rd group of every part of sample, and (1 title 2 of embodiment, concentration are 10 μ g/
ML), the mixed mark standard working solution I of 100 μ L (1 title 2 of embodiment, concentration are 10 μ g/mL) is added in the 4th group of every part of sample,
Then pre-treatment is carried out using 1 title 3 of embodiment, method is detected in 1 title 4 of embodiment.
The retention time at peak each in olive oil sample is compared with mark standard working solution I is mixed under same analysis condition
Compared with if retention time is consistent, for substance of the same race.Then, the sample average rate of recovery and relative standard deviation (RSD) are calculated.
Exist and C16:0M, C16:0E, C18:2M, C18:1M, C18:0M, C18:2E, C18 in Fig. 1 in olive oil sample:
The consistent substance of 1E, C18:0E retention time, can be qualitative, and average recovery rate and relative standard deviation (RSD) the results are shown in Table 2.
2 olive oil mark-on of table tests average recovery rate and relative standard deviation (%) (n=6)
Note: the outer data of 2 bracket of table are average recovery rate, and data are relative standard deviation (RSD) in bracket.
By data in table 2 as it can be seen that under three pitch-based spheres, the average recovery rate of 8 kinds of free fatty acid methyl esters and ethyl ester is equal
It is between 91.44%-100.19%, relative standard deviation is between 3.54%-8.49%, is illustrated using the method for the present invention
Free fatty acid methyl esters and ethyl ester in olive oil are detected, accuracy and precision are good.
In addition, there is also consistent with C14:0M and C17:0M retention time in mixed mark standard working solution II for olive oil sample
Substance, it was demonstrated that detection method stability is good, high reliablity.
Embodiment 3 is using fatty acid methyl ester and ethyl ester content in the method for the present invention detection olive oil sample
Using method in 1 title 7 of embodiment to free in 4 kinds of olive oil samples in the edible vegetable oil sample database of laboratory
Fatty acid methyl ester and ethyl ester content are measured.Two samples are taken in every kind of olive oil, each sample measures three times, are averaged
Value, see Table 3 for details and Fig. 2-5 for specific measurement result.
From Fig. 2-5 as it can be seen that existing and C16:0M, C16:0E, C18:2M, C18:1M, C18 in Fig. 1 in olive oil sample:
The consistent substance of 0M, C18:2E, C18:1E, C18:0E retention time, can be qualitative.In addition, olive oil sample there is also with it is mixed
Mark the consistent substance of C14:0M and C17:0M retention time in standard working solution II, it was demonstrated that detection method stability is good, reliability
It is high.
The content (means standard deviation, mg/kg) of free fatty acid methyl esters and ethyl ester in 3 olive oil of table
| Extra Virgin | Virgin oil | Mixed olive oil | Olea europaea fruit residual oil | |
| C16:0M | 20.01±1.03 | 20.45±0.37 | 10.04±7.74 | 22.45±10.14 |
| C16:0E | 16.80±0.81 | 19.89±2.32 | 31.20±7.30 | 63.81±15.41 |
| C18:2M | 9.91±1.66 | 8.93±1.41 | 1.04±1.47 | 26.10±11.86 |
| C18:1M | 50.3±14.04 | 60.51±8.50 | 24.02±9.49 | 123.58±49.24 |
| C18:0M | N.D. | 4.98±0.16 | 0.02±0.03 | 5.97±5.82 |
| C18:2E | N.D. | 4.27±0.84 | 18.13±2.13 | 108.72±43.10 |
| C18:1E | 3.95±3.01 | 30.13±4.77 | 62.87±1.92 | 574.78±261.75 |
| C18:0E | 8.35±0.46 | 10.43±1.69 | 19.82±5.98 | 41.10±5.07 |
| Ethyl ester summation | 29.10±4.27 | 64.71±9.61 | 132.02±17.32 | 788.40±325.34 |
| It amounts to | 109.32±15.62 | 159.57±0.52 | 167.13±33.11 | 966.50±402.39 |
By data in table 3 as it can be seen that the Extra Virgin sample free-fat acetoacetic ester of this laboratory sample database always contains
Amount is 29.1mg/kg, meets wanting for the fatty-acid ethyl ester content≤35mg/kg that dissociates in Extra Virgin in international standard
It asks.And virgin oil, mixed olive oil and olea europaea fruit residual oil middle reaches from fatty-acid ethyl ester total content 50mg/kg with
On, wherein olea europaea fruit residual oil middle reaches are up to 788.40mg/kg from fatty-acid ethyl ester total content, are the 27 of Extra Virgin
Times.
Claims (8)
1. a kind of quick environmental protection tests method of free fatty acid methyl esters and ethyl ester in olive oil, it is characterised in that including walking as follows
It is rapid:
(1) silicagel column Supelclean is usedTMLC-Si SPE carries out pre-treatment to olive oil sample；
(2) olive oil sample after pre-treatment is analyzed using gas-chromatography；
(3) content of free fatty acid methyl esters and ethyl ester in olive oil is calculated according to working curve.
2. according to claim 1 in olive oil free fatty acid methyl esters and ethyl ester quick environmental protection tests method, feature
It is that the free fatty acid methyl esters include methyl hexadecanoate, methyl stearate, methyl oleate and methyl linoleate, it is described free
Fatty-acid ethyl ester includes ethyl palmitate, ethyl stearte, ethyl oleate and ethyl linoleate.
3. the quick environmental protection tests method of free fatty acid methyl esters and ethyl ester in olive oil according to claim 1 or claim 2, special
Sign is that olive oil sample is transferred in the silicagel column activated with 6mL n-hexane in advance with 1-3mL n-hexane, uses 25-30mL
The mixed liquor of n-hexane and ether carries out chromatography eluant, collects eluent, removes solvent, then uses 1-3mL n-hexane dissolution.
4. according to claim 3 in olive oil free fatty acid methyl esters and ethyl ester quick environmental protection tests method, feature
It is that gas chromatography analysis method is as follows: the olive oil sample after pre-treatment is analyzed using DB-5HT gas chromatography；Capillary
Tubing string temperature program: initial temperature is 80 DEG C, rises to 140 DEG C with 40 DEG C/min heating rate, then with 5 DEG C/min heating
Rate rises to 335 DEG C, and in 335 DEG C of holding 20min；Injector temperature: 250 DEG C；Detector temperature: 350 DEG C；Carrier gas: helium
Gas；Flow rate of carrier gas: 1.0 mL/min；Sample volume: 1.0 μ L；Input mode: Splitless injecting samples.
5. according to claim 4 in olive oil free fatty acid methyl esters and ethyl ester quick environmental protection tests method, feature
It is that the working curve obtains with the following method: uses n-hexane to prepare for solvent and contain methyl hexadecanoate, stearic acid first
The mixed mark standard work of ester, methyl oleate, methyl linoleate, ethyl palmitate, ethyl stearte, ethyl oleate and ethyl linoleate
Make liquid I；The mixed mark standard working solution I is diluted to the mixed mark standard working solution of several various concentrations using n-hexane；It will be each
Mixed mark standard working solution is analyzed using gas-chromatography, using each aliphatic ester content as abscissa, with the gas of each aliphatic ester
Phase chromatographic peak area is ordinate mapping, draws working curve.
6. according to claim 5 in olive oil free fatty acid methyl esters and ethyl ester quick environmental protection tests method, feature
It is during obtaining working curve that gas chromatography analysis method is as follows: using the mixed mark mark of DB-5HT gas chromatography analysis
Quasi- working solution；Capillary column temperature program: initial temperature is 80 DEG C, rises to 140 DEG C with 40 DEG C/min heating rate, then
335 DEG C are risen to 5 DEG C/min heating rate, and in 335 DEG C of holding 20min；Injector temperature: 250 DEG C；Detector temperature:
350 ℃；Carrier gas: helium；Flow rate of carrier gas: 1.0 mL/min；Sample volume: 1.0 μ L；Input mode: Splitless injecting samples.
7. according to claim 6 in olive oil free fatty acid methyl esters and ethyl ester quick environmental protection tests method, feature
It is that olive oil sample before preceding processing, is added to and takes myristic acid methyl esters and methyl margarate.
8. detection method described in any one of claim 1 ~ 7 free fatty acid methyl esters and the qualitative inspection of ethyl ester in olive oil
Application in survey.
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Address after: Powerise 210019 Nanjing Road, Jiangsu province No. 39 Applicant after: Nanjing Customs animal and plant and food testing center Address before: Powerise 210019 Nanjing Road, Jiangsu province No. 39 Applicant before: ANIMALS, PLANTS AND FOOD INSPECTION CENTER OF JIANGSU ENTRY-EXIT INSPECTION AND QUARANTINE BUREAU |
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Application publication date: 20190524 |